CN102584086A - Preparation method for synthetizing high efficiency water reducing agent by 2-naphthol waste water - Google Patents
Preparation method for synthetizing high efficiency water reducing agent by 2-naphthol waste water Download PDFInfo
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- CN102584086A CN102584086A CN2012100117957A CN201210011795A CN102584086A CN 102584086 A CN102584086 A CN 102584086A CN 2012100117957 A CN2012100117957 A CN 2012100117957A CN 201210011795 A CN201210011795 A CN 201210011795A CN 102584086 A CN102584086 A CN 102584086A
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Abstract
The invention relates to a preparation method for synthetizing a high efficiency water reducing agent by 2-naphthol waste water. The invention belongs to the technical field of concrete water reducing agents. According to the preparation method for synthetizing the high efficiency water reducing agent by the 2-naphthol waste water, the proportion of crude naphthalene to concentrated sulfuric acid to naphthol waste water to formaldehyde is (1:0.8)-(1.0:0.1)-(0.9:0.5)-0.8. The preparation method for synthetizing the high efficiency water reducing agent by the 2-naphthol waste water comprises the following process flows of: 1-, sulfonating: heating to melt crude naphthalene, adding the concentrated sulfuric acid when the temperature rises to 130-160 DEG C, and reacting for 2-2.5 hours at the temperature of 160-165 DEG C; 2-, hydrolyzing: cooling reactants to 90-110 DEG C, adding naphthol waste liquor and hydrolyzing for 0.5-1 hour; 3-, condensation: dropwise adding the formaldehyde at the temperature of 95-115 DEG C and reacting for 3-6 hours; and (4) neutralizing: adding liquid caustic soda to neutralize a condensation compound to regulate a pH value to be 7-9 to obtain a water reducing agent product. The preparation method for synthetizing the high efficiency water reducing agent by the 2-naphthol waste water has the advantages that the production process is simple, the operation is convenient, the process control is easy, waste is turned into wealth, and thereby, secondary emission cannot be generated, and the economic value and the social benefit are high and the like.
Description
Technical field
The invention belongs to the cement water reducing agent technical field, particularly relate to a kind of preparation method of beta naphthal waste water synthesizing efficient water reducer.
Background technology
Cement water reducing agent is indispensable in a high performance concrete component, not only improves concrete performance, improves the quality of buildings, and can practice thrift cement widely, and manpower and material resources have very high value.
At present, the naphthalene water reducer turnout is maximum, uses the widest.Naphthalene series high-efficiency water-reducing agent accounts for more than 70% of water reducer consumption.Be characterized in that water-reducing rate is higher, not bleed, little to time of coagulation influence, better relatively with cement adaptability, can with the compound use of other various admixtures, price is also relatively cheap.
Beta naphthal is claimed β-Nai Fen again, is important Organic Chemicals and dyestuff intermediate, is mainly used in dyestuff, pigment dyestuff, rubber antioxidant and medicine and the pesticide industry.Traditional sulfonated alkali fusion method is produced beta naphthal; Be to be raw material with the refined naphthalene; Get the 2-naphthene sulfonic acid with 96%～98% sulfuric acid sulfonation, again with in the S-WAT with generate its sodium salt, get beta naphthal sodium with sodium hydroxide alkali fusion then; Then get the thick product of beta naphthal with sulfuric acid acidation, through boil, wash, dry, underpressure distillation gets the beta naphthal product.Operation is loaded down with trivial details, discharges great amount of wastewater in the production process.There is the waste strength height in production, toxicity is big, color and luster is dark, the soda acid resiliency strong, be difficult to biochemical degradation, and human body and environment are caused bigger technical problems such as harm.
CN1120030 has reported a kind of method of utilizing waste phenol dregs oil refinery synthesizing efficient water reducer; " utilizing the research of the synthetic FDN type efficient cement water reducing agent of naphthalene Residual oil " reported a kind of method of utilizing coal tar at 210 ℃-260 ℃ cut product synthesizing efficient water reducers, do not see the report that directly utilizes naphthols waste water synthesizing efficient water reducer.
Summary of the invention
The present invention provides a kind of preparation method of beta naphthal waste water synthesizing efficient water reducer for solving the technical problem that exists in the known technology.
The purpose of this invention is to provide that a kind of to have production process simple, easy to operate, technology controlling and process is easy; And turn waste into wealth; Do not need extras, do not have secondary emission, have the preparation method of the beta naphthal waste water synthesizing efficient water reducer of characteristics such as good economic worth and social benefit.
The present invention proposes a kind of method of utilizing beta naphthal to prepare high efficiency water reducing agent, and the discharging of using this method not only can solve oil refinery effluent to reach the purpose that control is polluted, can also obtain important cement additive-high efficiency water reducing agent.
Manufacturer all is that raw material is produced β-Nai Fen through sulfonation, alkali fusion with the refined naphthalene.Discharge the acid waste water of naphthene sulfonic acid in the production process, include sodium sulfate and the S-WAT of sodium naphthalene sulfonate 9000-13000mg/l and 6-10%, CODcr is about 30000mg/l, waste water complicated component, concentration height, dark, the difficult degradation of color and luster.
Operational path of the present invention is: sulfonation → hydrolysis → condensation → neutralization.Key of the present invention is to utilize the production β-Nai Fen as the hydrolysis water sulfonated naphthalene under the normal process to be hydrolyzed; Residual sodium naphthalene sulfonate in the waste water can be participated in next step condensation reaction, sodium sulfate and S-WAT also be in important component part in the dense or low dense naphthalene water reducer.
The technical scheme that the preparation method of beta naphthal waste water synthesizing efficient water reducer of the present invention takes for the technical problem that exists in the solution known technology is:
A kind of preparation method of beta naphthal waste water synthesizing efficient water reducer, it is characterized in that: preparing method's technical process may further comprise the steps; The each component weight ratio is a NAPTHALENE FLAKES. (INDUSTRIAL GRADE: the vitriol oil: naphthols waste water: formaldehyde=1: 0.8-1.0: 0.1-0.9: 0.5-0.8;
(1) sulfonation: with the NAPTHALENE FLAKES. (INDUSTRIAL GRADE heat fused, heat while stirring, when temperature is elevated to 130-160 ℃, add the vitriol oil, reaction is 2-2.5 hour under 160 ℃ of-165 ℃ of conditions;
(2) hydrolysis: the temperature of charge after the sulfonation is dropped to 90-110 ℃, add the naphthols waste liquid, hydrolysis 0.5-1 hour;
(3) condensation: under 95 ℃-115 ℃ temperature, drip formaldehyde, the reaction times is 3-6 hour;
(4) neutralization: add liquid caustic soda and make the neutralization of condenses alkali, the pH value is transferred to 7-9, obtain the water reducer product.
The preparation method of beta naphthal waste water synthesizing efficient water reducer of the present invention can also take following technical scheme:
The preparation method of described beta naphthal waste water synthesizing efficient water reducer is characterized in: the weight percent concentration of the vitriol oil is 95%-98%.
The preparation method of described beta naphthal waste water synthesizing efficient water reducer, be characterized in: the naphthols waste liquid contains sodium naphthalene sulfonate 9000-13000mg/l, the sodium sulfate of weight concentration 6-10% and S-WAT.
The preparation method of described beta naphthal waste water synthesizing efficient water reducer is characterized in: during condensation, the mol ratio of sodium naphthalene sulfonate and formaldehyde is 1: 0.6-1.1.
The preparation method of described beta naphthal waste water synthesizing efficient water reducer is characterized in: the weight percent concentration of formaldehyde is 30-40%.
The preparation method of described beta naphthal waste water synthesizing efficient water reducer is characterized in: liquid caustic soda is that concentration is the aqueous sodium hydroxide solution of 30-35%.
Advantage and positively effect that the present invention has are:
A kind of preparation method of beta naphthal waste water synthesizing efficient water reducer is owing to adopted brand-new technology scheme of the present invention; Compared with prior art; The present invention not only can dispose beta naphthal waste water under the condition that does not increase extra input and facility investment; And the high efficiency water reducing agent of producing has good dispersive ability, and its water-reducing rate can reach 15%-25%.The concrete incorporation degree of being mixed is good, does not grab at the end, and has good increase effect.It is simple that the present invention has production process, easy to operate, and technology controlling and process is easy, and turn waste into wealth, and do not need extras, do not have secondary emission, has advantages such as good economic worth and social benefit.
Embodiment
For further understanding technology contents of the present invention, characteristics and effect, the following examples of giving an example now specify as follows:
Embodiment 1
The preparation method of beta naphthal waste water synthesizing efficient water reducer; In having the four-hole boiling flask of stirring, drop into NAPTHALENE FLAKES. (INDUSTRIAL GRADE 500g, drip 98% vitriol oil 460g when being heated to 140 ℃, and under 160 ℃-165 ℃ condition, be incubated 2.5 hours;, temperature adds beta naphthal waste water 220g when reducing to 100 ℃; Hydrolysis 1 hour, insulation drips 37% formaldehyde solution and is incubated 5 hours down at 95 ℃-105 ℃, after condensation finishes; It is cooled to room temperature and adds 32% liquid caustic soda to be neutralized to PH be 8, obtain final product high efficiency water reducing agent.
Embodiment 2
The preparation method of beta naphthal waste water synthesizing efficient water reducer; In the four-hole boiling flask that has stirring, drop into NAPTHALENE FLAKES. (INDUSTRIAL GRADE 500g, drip 98% vitriol oil 500g when being heated to 140 ℃, and under 160 ℃-165 ℃ condition, be incubated 2 hours;, temperature adds beta naphthal waste water 200g when reducing to 100 ℃; Hydrolysis 0.5 hour, insulation drips 37% formaldehyde solution and is incubated 4 hours down at 95 ℃-105 ℃, after condensation finishes; It is cooled to room temperature and adds 32% liquid caustic soda to be neutralized to PH be 8, obtain final product high efficiency water reducing agent.
Embodiment 3
The preparation method of beta naphthal waste water synthesizing efficient water reducer; In the four-hole boiling flask that has stirring, drop into NAPTHALENE FLAKES. (INDUSTRIAL GRADE 500g, drip 98% vitriol oil 500g when being heated to 140 ℃, and under 160 ℃-165 ℃ condition, be incubated 2 hours;, temperature adds 100g water and beta naphthal waste water 100g when reducing to 100 ℃; Hydrolysis 0.5 hour, insulation drips 37% formaldehyde solution and is incubated 5 hours down at 95 ℃-105 ℃, after condensation finishes; It is cooled to room temperature and adds 32% liquid caustic soda to be neutralized to PH be 8, obtain final product high efficiency water reducing agent.
Implementation result
Below the table 1. be performance condition of the present invention and with each item performance comparison of other like product
Table 1 is the water reducer performance index of the present invention's preparation.Quality monitoring testing station the 24 station check through Tianjin, institute's inspection project meet GB8076-2008 " concrete admixture ", GB18588-2001 " discharging limiting the quantity of of ammonia in the concrete admixture " standard.
The water reducer of table 2. the present invention preparation and the performance comparison of other naphthalene series high-efficiency water-reducing agent
Table 2 is the water reducer of the present invention's preparation and the performance comparison of other naphthalene series high-efficiency water-reducing agent, and volume is folding solid 0.75%.Can find out that from test-results the high efficiency water reducing agent of the inventive method preparation is approaching with the high efficiency water reducing agent performance of producing with NAPTHALENE FLAKES. (INDUSTRIAL GRADE, particularly aspect workability of concrete and intensity, has good dispersing property and ultimate compression strength.
Claims (6)
1. the preparation method of a beta naphthal waste water synthesizing efficient water reducer, it is characterized in that: preparing method's technical process may further comprise the steps; The each component weight ratio is a NAPTHALENE FLAKES. (INDUSTRIAL GRADE: the vitriol oil: naphthols waste water: formaldehyde=1: 0.8-1.0: 0.1-0.9: 0.5-0.8;
(1) sulfonation: with the NAPTHALENE FLAKES. (INDUSTRIAL GRADE heat fused, heat while stirring, when temperature is elevated to 130-160 ℃, add the vitriol oil, reaction is 2-2.5 hour under 160 ℃ of-165 ℃ of conditions;
(2) hydrolysis: the temperature of charge after the sulfonation is dropped to 90-110 ℃, add the naphthols waste liquid, hydrolysis 0.5-1 hour;
(3) condensation: under 95 ℃-115 ℃ temperature, drip formaldehyde, the reaction times is 3-6 hour;
(4) neutralization: add liquid caustic soda and make the neutralization of condenses alkali, the pH value is transferred to 7-9, obtain the water reducer product.
2. according to the preparation method of the described beta naphthal waste water of claim 1 synthesizing efficient water reducer, it is characterized in that: the weight percent concentration of the vitriol oil is 95%-98%.
3. according to the preparation method of the described beta naphthal waste water of claim 1 synthesizing efficient water reducer, it is characterized in that: the naphthols waste liquid contains sodium naphthalene sulfonate 9000-13000mg/l, the sodium sulfate of weight concentration 6-10% and S-WAT.
4. according to the preparation method of the described beta naphthal waste water of claim 3 synthesizing efficient water reducer, it is characterized in that: during condensation, the mol ratio of sodium naphthalene sulfonate and formaldehyde is 1: 0.6-1.1.
5. according to the preparation method of claim 1 or 4 described beta naphthal waste water synthesizing efficient water reducers, it is characterized in that: the weight percent concentration of formaldehyde is 30-40%.
6. according to the preparation method of the described beta naphthal waste water of claim 1 synthesizing efficient water reducer, it is characterized in that: liquid caustic soda is that concentration is the aqueous sodium hydroxide solution of 30-35%.
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103172293A (en) * | 2013-03-25 | 2013-06-26 | 萧县鑫固混凝土外加剂有限公司 | Technical formula and production technology for preparing naphthalene-based superplasticizer |
| CN105461252A (en) * | 2015-11-27 | 2016-04-06 | 中蓝连海设计研究院 | Method for preparation of naphthalene dispersing agent by using naphthalenesulfonate recycled waste liquid and use of naphthalene dispersing agent |
| CN105884238A (en) * | 2015-08-18 | 2016-08-24 | 科之杰新材料集团有限公司 | Naphthalene-based powder water reducing agent and preparation method thereof |
| CN106348634A (en) * | 2016-08-24 | 2017-01-25 | 安徽鑫固环保股份有限公司 | Modified amino high efficiency water reducing agent prepared from 2-naphthol wastewater and preparation method thereof |
| CN107573471A (en) * | 2017-08-31 | 2018-01-12 | 浙江吉盛化学建材有限公司 | A kind of production technology of FDN high efficiency water reducing agents |
| CN108409181A (en) * | 2018-05-18 | 2018-08-17 | 萧县沃德化工科技有限公司 | A kind of modified aliphatic water reducing agent of useless residue in the production process containing phenols |
| CN108484852A (en) * | 2018-05-18 | 2018-09-04 | 萧县沃德化工科技有限公司 | A kind of modified naphthalene series water-reducing agent of useless residue in the production process containing phenols |
| CN108503254A (en) * | 2018-05-18 | 2018-09-07 | 萧县沃德化工科技有限公司 | A kind of useless rosin in adhesive production process is used for modified naphthalene series water-reducing agent |
| CN108609887A (en) * | 2018-05-18 | 2018-10-02 | 萧县沃德化工科技有限公司 | The method that the spent lye of mercerization prepares modified naphthalene series water-reducing agent |
| CN110981059A (en) * | 2019-12-09 | 2020-04-10 | 常州中源工程技术有限公司 | System and process for treating waste water containing sodium sulfate salt and sodium sulfite salt dinaphthol |
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Cited By (13)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103172293A (en) * | 2013-03-25 | 2013-06-26 | 萧县鑫固混凝土外加剂有限公司 | Technical formula and production technology for preparing naphthalene-based superplasticizer |
| CN105884238A (en) * | 2015-08-18 | 2016-08-24 | 科之杰新材料集团有限公司 | Naphthalene-based powder water reducing agent and preparation method thereof |
| CN105884238B (en) * | 2015-08-18 | 2017-12-22 | 科之杰新材料集团有限公司 | A kind of naphthalene system pulvis water reducer and preparation method thereof |
| CN105461252A (en) * | 2015-11-27 | 2016-04-06 | 中蓝连海设计研究院 | Method for preparation of naphthalene dispersing agent by using naphthalenesulfonate recycled waste liquid and use of naphthalene dispersing agent |
| CN106348634B (en) * | 2016-08-24 | 2019-01-01 | 安徽鑫固环保股份有限公司 | A kind of waste liquid modified aminosulfonate-based superplasticizer of beta naphthal and preparation method thereof |
| CN106348634A (en) * | 2016-08-24 | 2017-01-25 | 安徽鑫固环保股份有限公司 | Modified amino high efficiency water reducing agent prepared from 2-naphthol wastewater and preparation method thereof |
| CN107573471A (en) * | 2017-08-31 | 2018-01-12 | 浙江吉盛化学建材有限公司 | A kind of production technology of FDN high efficiency water reducing agents |
| CN107573471B (en) * | 2017-08-31 | 2019-10-29 | 浙江吉盛化学建材有限公司 | A kind of production technology of FDN high efficiency water reducing agent |
| CN108409181A (en) * | 2018-05-18 | 2018-08-17 | 萧县沃德化工科技有限公司 | A kind of modified aliphatic water reducing agent of useless residue in the production process containing phenols |
| CN108609887A (en) * | 2018-05-18 | 2018-10-02 | 萧县沃德化工科技有限公司 | The method that the spent lye of mercerization prepares modified naphthalene series water-reducing agent |
| CN108503254A (en) * | 2018-05-18 | 2018-09-07 | 萧县沃德化工科技有限公司 | A kind of useless rosin in adhesive production process is used for modified naphthalene series water-reducing agent |
| CN108484852A (en) * | 2018-05-18 | 2018-09-04 | 萧县沃德化工科技有限公司 | A kind of modified naphthalene series water-reducing agent of useless residue in the production process containing phenols |
| CN110981059A (en) * | 2019-12-09 | 2020-04-10 | 常州中源工程技术有限公司 | System and process for treating waste water containing sodium sulfate salt and sodium sulfite salt dinaphthol |
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Application publication date: 20120718 |